Apparatus for making halogenated products



jan. 2

PANY, 0F MID, MICHIGAN,

E.- T, 01 SAGINAW, MICHIGAN, .ASSIGNOR TO THE DOW CE I car. com A conro'rron or meme.

APPARATUS FOR MAKING HALOGENA'IED BBODUCTS.

Application med October 17, 1919. Serial No. 881,446.

To all whom it may concern:

Be it known that 1, WILLIAM E. Kms'r,

a citizen of the United States and aresi-' passing hydrogc dent of Saginaw, county of aginaw, and State of Michigam-have invented a new and useful Improvement in Apparatus for Making Halogenated Products, of which the following is a specification, the rmciple of the invention bein herein exp ained and the best mode in w 'ch I have contemplated applying that principle, so as to distinguish it. from other inventions.

The resent improvements, relatln as indicate to the manufacture of alogenated products, have regard more articularly to the manufacture of chlorinated- (or brominated) derivatives of eth Iene, e. 1 col chlorhydrin (C CIILQ or CHCL% OH). Compounds of this character are sometimes referred to as halogen hydrins by way of general deslgnation, it being understood that other halogen derivatives, as well as chlorhydrins, may be made by the same method or process, and employing the same or similar apparatus as that hereinafter described. P

Approved methods for obtaining ch1or-- hydrin, as described in'the texts (e. g. see Bernthsens Organic Chemistry), include 11 chloride into warm glycol, and the addition of hypochlorous acid to ethylene. The object of the present invention is the production of such chlorhydrm or related halogen derivative as directly as possible from the halogen and eth lens, and while a hypohalogenous acid may e formed as an intermediate, the reactions occur practicall continuously, and it is not required to andle the acid as such. 7

To the accomplishment of the foregoing and related ends, the invention, then, c'onsists of the means hereinafter full described and particularly pointed out in the claims, the annexed dra and: the following description setting orth in detail one type of apparatus embodying the mvention, such disclosure,howev er, constltuting but one of various ways m which the principle of the invention may be used. I

In said annexed drawing The single figure there appearing illustrates, in a more or less dla'grammatic fashion, an arrangement of apparatusembodymg m present improvements. Y As lustrated in the drawing in question,

the principal element of the apparatus is a suitably lined horizontal cylin r'ical stationary absorber 1 equipped with an agitator in.

the form of a series of paddles 2 carried by an axial shaft 3 rovided with a, driving pulley 4 exterior 0 one end of the absorber.

uitable pipes 5 and 6, havingl perforated extensions y disposed within the chamber along its bottom wall provide means for introducing ethylene and chlorine as indicated. Connected-with the upper wall of the absorber by means of a and 8 respective suitable pi e 9 is a separating chamber 10,

through w ich gas may be drawn ofi without interrupting operation of the absorber, while any li nor that is carried along with such gas is a lowed to run back through another connection 11. A sight glass 12 at one end of the absorber chamber serves to indicate the liquid level within the latter.

Leadin from the bottom of the absorber chamber 1s a valve controlled'discharge 13, through which the liquid contents 0 chamber may be conducted to a; neutralizing chamber 14 of any suitable construc- .tion. From the latter in turn the liquid ma be transferred through a valve-contro ed pipe 15 to a suitable still 16, having connected therewith a condenser 17 Having thus described the arrangement of apparatus, the operation thereof may be now set forth. The ethylene and chlorine are passed, as reviousl indicated through pipes 5 and 6 into the c osed absor or or reaction chamber. Here the two mutually dissolve and react 'accor to the following equations ply of eth lene and chlorine is then shut o and the r e is run to the neutralizing tank or cham r 14, where the hydrochloric acid in such char is removed with lime. The transfer of .t 0 charge from the absorber to the neutralizer may be facilitated by admitting a suitable gas under-pressure a 0 vs the same through a valve-controlled pipe 18 provided for the purpose. The neutralized char is next transferred to still 16 and listed throughcol 17 which readily permits the securin of a forty per cent 0 orhydrin portion. uch portion can then be subjected to further purification or concentration, this, however, forming no part of the present invention,

It will be observed that an unusually high concentration of chlorhydrin is obtainable by the use of the foregomg process and apparatus. It is also unnecessary to have an ase present in the reaction, the latter in e that such process is not necessarily limited drins,

to the particular olefin, viz, ethylene, from which this compound is derived but that other of the gaseous and volatile olefins, such as propylene, the etc., hereinafter referred to generally as olefinic bodies, so far as the are capable of producing compounds oft e class of chlorhydrin may be similarly utilized in the manner described. On the other hand, as previously indicated, such apparatus is equally adaptable for the manufacture of other. halohydrins, and particularly of bromhysince bromine in vapor form can of course be introduced into the absorber in the same fashion as chlorine gas and the remaining steps of the operation-will follow in the same sequence.

Other-modes of applying the principle of butylenes, the amylenes,

lo ed instead of my invention may be em y mg hade as rethe one explained, change gards the mechanism I vided the means stated by any of the fol ow ing claims or the equivalent of such stated .pipes for supplying a halogen and an olefinic body to said chamber, said pipes having perforated extensions, respectively, disposfid within said chamber along its lower wa v 2. In an apparaus for making halogenated products, he combination of a horizontal cylindrical stationary absorbing chamber, a. se arator connected with the upper wall of said chamber, an agitator comprising an axial shaft within said chamber and a series of paddles carried by said shaft, andseparate pipes for. supplyin a halogen and an olefinic bod to said c amber, said pipes having per orated extensions, respectively,

disposed within said chamber along itslower wall. 4

Signed by me this 9th day of October,

WILLIAM E. KIRST.

herein *d1sclosed,.. ro- 

